Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
  • C08J5/18—Manufacture of films or sheets
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
  • C09J7/00—Adhesives in the form of films or foils
  • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
  • C09J7/22—Plastics; Metallised plastics
  • C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
  • C09J7/241—Polyolefin, e.g.rubber
  • C09J7/243—Ethylene or propylene polymers
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
  • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
  • C08J2323/10—Homopolymers or copolymers of propene
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K5/00—Use of organic ingredients
  • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
  • C08K5/0083—Nucleating agents promoting the crystallisation of the polymer matrix
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
  • C09J2301/00—Additional features of adhesives in the form of films or foils
  • C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
  • C09J2301/41—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the carrier layer

Definitions

• the invention relates to a carrier film made of polypropylene, a process for producing the same and the use of these in an adhesive tape.
• Films with high longitudinal strength are usually achieved by stretching extruded flat films of semi-crystalline thermoplastics. This is predominantly a biaxial stretching, in exceptional cases, the films are oriented to further increase the longitudinal tensile strength only in the longitudinal direction.
• both conventional biaxially oriented and monoaxially stretched films based on polypropylene have low tear propagation strengths in the transverse direction, in contrast to unstretched films from the blown or cast process.
• injured edges of the film or the adhesive tape (caused by blunt knives when cutting or later unintentional injury to the cut edge) easily lead to entrapment under tensile load.
• filaments or nets made of filaments of glass or plastic.
• the production of such Filamentklebeb is very complex on the system side and thus expensive and prone to failure.
• the filaments and laminating adhesive or an additional pressure-sensitive adhesive coating
• Further disadvantages of such filament adhesive tapes are low kink resistance, high thickness, unclean cutting edges and lack of weldability and lack of recyclability. The production is for example in the US 4,454,192 A described.
• the DE 21 04 817 A1 describes a process for producing a tape carrier of polyolefin (polyethylene or polyethylene). By stretching in the longitudinal direction, a tensile strength in the longitudinal direction of 320 N / mm 2 should be achieved (according to a preferred embodiment). Stretching ratio and tension reached at 10% elongation are not disclosed.
• Subject of the EP 0 255 866 A1 is a longitudinally oriented or biaxially oriented polypropylene film of a polypropylene homopolymer or a polypropylene copolymer.
• the addition of elastomeric components increases the impact resistance in the transverse direction.
• This measure leads to a deterioration in the tensile strength and the tear propagation resistance in the transverse direction, since this prevents the formation of fibrous structures when the film is loaded in the transverse direction.
• the stretching ratio in the longitudinal direction is 1: 5.5 to 1: 7.
• Tensile strengths of 12 to 355 N / mm 2 are achieved. Values for the stresses at 10% elongation are not known.
• a tearing strip with reduced tear tendency is described by using a longitudinally stretched film made by co-extruding raw materials of different toughness.
• the tough coextrusion layer reduces the formation of microcracks when cutting the product, thereby improving the side tear strength. However, it does not avoid the tearing off of subsequently injured edges.
• the specified raw materials as the main component of the coextrusion layer serve to increase the toughness of this layer, but also lead to a significantly reduced tensile strength of the films in the longitudinal direction.
• the films described in the examples have the equivalent of a tensile strength of only 215 N / mm 2 .
• the recipe combination of PP block copolymer with a maximum of 20% ethylene and impact modifier is responsible for this.
• LLDPE low density polyethylene
• EVA EVA
• SBS rubber SBS rubber
• the strip has no high tear strength in the transverse direction.
• the stretch ratio is 1: 7.5.
• the Tensile stress at 10% elongation is 84 to 103 N / mm 2 and the tensile strengths are in the range of 196 to 214 N / mm 2 .
• the DE 44 02 444 A1 relates to a tear-resistant adhesive tape based on monoaxially oriented polyethylene.
• polyethylene has significantly lower heat resistance than PP, which can be detrimental both in the manufacture of the adhesive tape (drying of adhesive or other layers in the oven) and in later packaging applications such as grip tape, carton sealing tape, tear strips or paperboard reinforcing strips.
• the adhesive tapes on the cartons often become hot, for example, when passing through printing presses or after being filled with hot goods (for example, food).
• the US 5,145,544 A and the US 5,173,141 A describe an adhesive tape of a monoaxially stretched film having a rib structure for reinforcement, the ribs protruding partially from the surface, being partially embedded in the film surface, and having kerfs formed between the film and ribs.
• the film achieves high side tear strength, the tensile strength and ductility, however, are still in need of improvement.
• the essential shortcoming, however, is that such a film can not be produced on a production scale. The reasons for this are the poor stretchability in the usual width and an extremely poor flatness, so that the coatability with pressure-sensitive adhesive is no longer guaranteed.
• the flatness also deteriorates due to uneven and insufficient adhesion (due to the non-planar film) on the stretching rollers in the subsequent drawing process.
• the film is held in the middle region on the stretching rolls in the transverse direction, whereby the rib structure is changed by stretching and the overall product quality is inhomogeneous.
• Another disadvantage is the need for at least 50% embedding of the ribs by a calender, which is very expensive in the investment and makes the process much more complex.
• the surface ridge structure also tends to cause coating defects when applying release agents or primers to adhesive tape as the application methods for films require a smooth surface.
• Imprints of reinforcing filaments or rib structures in the surface of films are detrimental to printing, which requires smooth surfaces.
• the printability for the customer is an important criterion.
• a draw ratio of 1: 7 and tensile strengths of 157 to 177 N / mm 2 can be taken out; stresses at 10% elongation are not determined.
• a Stretching ratios of 1: 6.1 to 1: 7 and tensile strengths of up to 245 N / mm 2 can be deduced, stresses at 10% elongation are not determined.
• the EP 1 101 808 A1 tried to eliminate the disadvantages mentioned by the rib structures were moved into the interior of the film.
• the film has plane-parallel outer sides and contains at least two co-extruded layers of different composition whose boundary surface is not flat, but in cross-section has a non-straight boundary, which continues laminar in the longitudinal direction.
• the particular internal structure of the film is based on the fact that the thickness of a layer in the transverse direction varies periodically or irregularly and the second layer compensates for the thickness variations such that the total thickness is substantially constant. All the films mentioned have improved tensile strength and improved modulus of elasticity in the longitudinal direction compared to a normal adhesive tape.
• the stretching ratios are between 1: 6.7 and 1: 8.7.
• Tensile strengths are reached from 202 to 231 N / mm 2 and stresses at 10% elongation from 103 to 147 N / mm 2 .
• the EP 0 353 907 A1 applies the idea of fibrillating foils.
• an adhesive tape which is produced from a carrier layer which is adhesively bonded to a further layer of a fibrillated polymer film. Subsequently, the fibrillated side is coated with adhesive.
• the polymer film to be fibrillated is preferably extruded, consists of PP and is then monoaxially stretched in the machine direction. This likewise very complicated process has the disadvantage that the laminate must be produced in four process steps (extrusion, stretching, fibrillation and bonding of the fibrils on the BOPP carrier film).
• the thickness of the films of EP 0 353 907 A1 is about 25 microns (BOPP) and about 5 microns (stretched PP film). Therefore, only tensile strengths of 99 to 176 N / cm and tear strengths of 15 to 22 N / cm can be achieved at.
• the object of the invention is to provide a carrier film available that does not or not to the extent shows the disadvantages of the prior art. In particular, this should have a high tear propagation resistance in the transverse direction and be transparent.
• the invention relates to a carrier film which contains at least one polypropylene and which is monoaxially stretched in the longitudinal direction. It is essential to the invention that at least one nucleating agent is homogeneously distributed in the carrier film.
• the film Due to the combination according to the invention of a homogeneously distributed nucleating agent with a monoaxial orientation, the film has a crystal-clear appearance and, if no additional pigments or dyes are added, is colorless.
• the film surface is preferably high gloss.
• Nucleating agents are nucleating agents (salts of organic acids, for example sodium benzoate) which are added to crystallizable thermoplastics, especially polyolefins, polyesters, polyamides, etc., in order to accelerate the crystallization. By changing the crystallization process, products with altered physical properties are created.
• homogeneous distribution is meant the distribution in a layer.
• the carrier film may well have several layers, which are homogeneous in terms of the respective concentration of the nucleating agent in itself. However, the layers may well have different concentration of nucleating agent.
• the carrier film has a haze of at most 30%, preferably at most 15% and / or a gloss of at least 70%, preferably of at least 120%.
• the test methods for determining these values are explained below.
• the stretching process conditions are preferably chosen so that the stretch ratio is the maximum technically feasible for the primary film.
• the draw ratio is at least 1: 8, preferably at least 1: 9.5 in the longitudinal direction.
• the draw ratio indicates that at a stretch ratio of 1: 8, a section of 8 m length of the stretched film is produced from a section of the film of, for example, 1 m in length.
• the stretch ratio is also defined as the quotient of the line speed to the stretching roller speed.
• the carrier film has a tension in the machine direction at 1% elongation of at least 20, preferably at least 40 N / mm 2 and / or a stress at 10% elongation of at least 250, preferably at least 300 N / mm 2 .
• the tensile strength is more preferably at least 300, more preferably at least 350 N / mm 2 .
• the tear propagation resistance in the transverse direction with respect to the film thickness preferably reaches at least 450 N / mm 2 .
• the width-related force values are divided by the thickness. In the case of a determination on an adhesive tape produced with the carrier film, the thickness should not be based on the total thickness, but only on the carrier film.
• the thickness of the carrier film is preferably between 25 and 200, more preferably between 40 and 140, most preferably between 50 and 90 microns.
• Suitable film raw materials according to this invention are commercially available polypropylene homopolymers or polypropylene copolymers.
• the melt indices of the above polymers should be in the range suitable for flat film extrusion. This range is according to a preferred embodiment between 0.3 and 15 g / 10min, preferably in the range of 0.8 and 5 g / 10min (measured at 230 ° C / 2.16kg).
• the flexural modulus according to a further advantageous embodiment is at least 1000, preferably at least 1500, more preferably at least 2000 MPa.
• the polypropylene is preferably predominantly isotactic.
• the polymers for forming the carrier film can be present in pure form or in blends with additives such as antioxidants, light stabilizers, antiblocking agents, lubricants and processing aids, fillers, dyes or pigments.
• additives such as antioxidants, light stabilizers, antiblocking agents, lubricants and processing aids, fillers, dyes or pigments. The addition should be avoided or reduced to the extent necessary to not (significantly) degrade the optical properties.
• the highly transparent or high-gloss appearance is achieved as described by the addition of at least one nucleating agent.
• nucleating agent all suitable for polypropylene nucleating agents can be used. Particularly suitable are nucleating agents which produce ⁇ - or ⁇ -crystals.
• organic nucleating agents such as benzoates, phosphates or sorbitol derivatives are used.
• nucleating agents are for example in Chapter "9.1 Nucleating Agents” in Ullmann's Encyclopaedia of Industrial Chemistry (Edition 2002 by Wiley-VCH Publishers, Article Online Posting Date June 15, 2000 ) or in the examples of US 2003195300 A1 ( US 6,927,256 B ).
• Another suitable measure is the use of a semicrystalline branched or coupled polymeric nucleating agent, as described in US Pat US 2003195300 A1 for example, a 4,4'-oxydibenzenesulfonyl azide modified polypropylene.
• the nucleating agent can be used in pure form or as a masterbatch.
• the manufacturing process can be controlled more safely if a compound of nucleating agent and polypropylene is used by the polymer manufacturer for the carrier production. It is preferable to use a polypropylene which has been finished nucleated by the polymer manufacturer.
• the screw of the extruder preferably contains a sufficient number or sufficiently intense mixing elements, since otherwise the nucleating agent could be distributed to inhomogeneous.
• the film may have been produced in one or more layers, preferably it is single-layered.
• the films may be modified by lamination, embossing or radiation treatment.
• the undrawn primary film with the nucleating agents does not have a crystal clear appearance. Only by the stretching in the longitudinal direction, this arises.
• the films can be provided with surface treatments. These are, for example, for bonding corona, flame, fluorine or plasma treatment or coatings of solutions, dispersions or liquid radiation-curable materials. Further possible coatings are printing and non-stick coatings, for example those of crosslinked silicones, acrylates (for example Primal® 205), polymers with vinylidene chloride or vinyl chloride as monomer or stearyl compounds such as polyvinyl stearyl carbamate of the chromium stearate complexes (for example Quilon® C) or reaction products of maleic anhydride copolymers and stearylamine ,
• the carrier film is preferably provided on one or both sides with an adhesive, preferably with a self-adhesive or a heat-activatable adhesive layer.
• adheresive tape encompasses all flat structures such as films or film sections which are expanded in two dimensions, tapes of extended length and limited width, tape sections, diecuts, labels and the like.
• the adhesive is preferably pressure-sensitive adhesive.
• the film is coated on one or both sides with the preferred pressure-sensitive adhesive as a solution or dispersion or 100% (for example melt) or by coextrusion with the film.
• the adhesive layer (s) can be crosslinked by heat or high-energy radiation and, if necessary, covered with release film or release paper.
• Suitable pressure sensitive adhesives are described in D. Satas, Handbook of Pressure Sensitive Adhesive Technology (Van Nostrand Reinhold).
• pressure-sensitive adhesives based on acrylate, natural rubber, thermoplastic styrene block copolymer or silicone are suitable.
• the self-adhesive composition used may preferably be blended with one or more additives such as tackifiers (resins), plasticizers, fillers, pigments, UV absorbers, light stabilizers, aging inhibitors, crosslinking agents, crosslinking promoters or elastomers.
• additives such as tackifiers (resins), plasticizers, fillers, pigments, UV absorbers, light stabilizers, aging inhibitors, crosslinking agents, crosslinking promoters or elastomers.
• Suitable elastomers for blending are, for example, EPDM or EPM rubber, polyisobutylene, butyl rubber, ethylene-vinyl acetate, hydrogenated block copolymers of dienes (for example by hydrogenation of SBR, cSBR, BAN, NBR, SBS, SIS or IR; Example known as SEPS and SEBS) or acrylate copolymers such as ACM.
• Tackifiers are, for example, hydrocarbon resins (for example, unsaturated C 5 or C 7 monomers), terpene-phenolic resins, terpene resins from raw materials such as ⁇ - or ⁇ -pinene, aromatic resins such as cumarone-indene resins or resins of styrene or ⁇ -methylstyrene such as rosin and its derivatives, such as disproportionated, dimerized or esterified resins, whereby glycols, glycerol or pentaerythritol can be used, as well as others as described in US Pat Ullmann's Encyclopedia of Industrial Chemistry, volume 12, pages 525 to 555 (4th edition), Weinheim , are listed. Particularly suitable are age-stable resins without olefinic double bond such as hydrogenated resins.
• Fillers and pigments such as carbon black, titanium dioxide, calcium carbonate, zinc carbonate, zinc oxide, silicates or silicic acid may be used, but should be avoided because of the lack of transparency.
• Suitable UV absorbers, light stabilizers and aging inhibitors for the adhesives are the same as those listed for the stabilization of the film.
• Suitable plasticizers are, for example, aliphatic, cycloaliphatic and aromatic mineral oils, di- or poly-esters of phthalic acid, trimellitic acid or adipic acid, liquid rubbers (for example nitrile or polyisoprene rubbers), liquid polymers of butene and / or isobutene, acrylic esters, polyvinyl ethers, liquid and soft resins based on the raw materials to adhesive resins, wool wax and other waxes or liquid silicones.
• liquid rubbers for example nitrile or polyisoprene rubbers
• liquid polymers of butene and / or isobutene acrylic esters
• polyvinyl ethers polyvinyl ethers
• liquid and soft resins based on the raw materials to adhesive resins, wool wax and other waxes or liquid silicones.
• Crosslinking agents are, for example, phenolic resins or halogenated phenolic resins, melamine and formaldehyde resins.
• Suitable crosslinking promoters are, for example, maleimides, allyl esters, such as triallyl cyanurate, polyfunctional esters of acrylic and methacrylic acid.
• the pressure-sensitive adhesive consists of light and transparent raw materials.
• Particularly preferred are acrylic pressure-sensitive adhesives (for example as a dispersion) or pressure-sensitive adhesives of styrene block copolymer and resin (as are customary, for example, for hot melt pressure sensitive adhesives).
• the coating thickness with adhesive is preferably in the range from 18 to 50, in particular 22 to 29 g / m 2 .
• the width of the adhesive tape rolls is preferably in the range of 2 to 60 mm.
• the carrier film according to the invention is particularly suitable for high-quality packaging applications. According to the prior art, no adhesive tapes have been found with monoaxially stretched in the longitudinal direction carrier film, which are highly transparent. Colorless monoaxially stretched carrier films are prepared from polypropylene block copolymer having a volume turbidity and have a slightly matt surface. Colorless monoaxially stretched carrier films are also partially made from a blend of polypropylene block copolymer or polypropylene homopolymer with polyethylene such as LLDPE or SBS rubber. It is well known to the person skilled in the art that colorless products of polypropylene block copolymer are slightly dull and cloudy; this effect is even more pronounced in the case of blends of polypropylene homopolymer and another polyolefin.
• biaxially stretched polypropylene films which have a high transparency.
• Transparent biaxially stretched films have long been used in packaging applications and also as adhesive tape carriers. They contain no nucleating agents, but get their transparency through the manufacturing process. These films have a low turbidity, since for their preparation fillers must be used as antiblocking agents.
• adhesive tapes with high demands on tensile strength and bending stiffness these biaxially stretched films are not suitable, since the orientation in the longitudinal direction is small compared to monoaxially stretched films.
• biaxially stretched films are generally offered between 15 and 35 ⁇ m. Unbulte films with thicknesses up to 60 microns are known, but difficult to produce. Monoaxially stretched adhesive tape films are usually used in the thickness range of 40 to 140 microns and therefore have the thickness particularly high strength.
• the appearance in the present invention is preferably achieved by a very homogeneously distributed nucleating agent.
• Antiblocking agents or other fillers are not needed in contrast to biaxially stretched films and should therefore not be used.
• the film has a high tensile strength and a high stress at 10% elongation.
• the film is stretched so much that the impact resistance across becomes very low. This may be detrimental to some applications, such as tear strips or carton closure, for applications such as reinforcement of die cut to cartons, it has been found to be advantageous.
• a slight elongation due to high longitudinal stretching avoids the tearing of cardboard cardboard (for example on punched carrying handles).
• Such films tend to fibrillate in the longitudinal direction, which prevents the tearing in the transverse direction by deflection of the crack in the longitudinal direction in the case of edge damage.
• BA 110 CF PP block copolymer, MFI 0.85 g / 10 min, not nucleated, flexural modulus 1200 MPa (Borealis) Moplen HP 501 D: homopolymer, MFI 0.7 g / 10 min, not nucleated, flexural modulus 1450MPa (Basell) Bormod HD 905: homopolymer, MFI 6 g / 10 min, flexural modulus 2150 MPa (Basell), contains, according to our analysis, a phosphate-based ⁇ -nucleant, probably ADK STAB NA-11 (Adeka Palmarole) Inspire D 404.01: MFI 3 g / 10 min, nucleated, flexural modulus 2068 MPa (Dow Chemical) nucleated (with a polymeric nucleating agent according to the US2003195300 A1 ) BNX BETAPP-N: ⁇ -nucleating agent in polypropylene, MFI 4 g / 10 min (Mayzo)
• the film was produced on a single-flute single-flute extrusion line with a flexible die-lip die, followed by a chill roll station and a one-step short-gap stretch line.
• Inspire D 404.01 was used as raw material Inspire D 404.01.
• the die temperature was 235 ° C
• chill roll temperatures and draw roll temperatures were adjusted to maximize the crystallinity of the film before and after the stretching operation.
• the stretch ratio was 1:10.
• the film was corona pretreated on both sides, coated on top with a 0.5% solution of PVSC in toluene as a release and dried.
• the adhesive was made from 42% by weight of SIS elastomer, 20% by weight of pentaerythritol ester of hydrogenated rosin, 37% by weight of a C 5 hydrocarbon resin having an R & B value of 85 ° C. and 1% by weight of Irganox antioxidant ® 1010 mixed in the melt and applied at 150 ° C with a nozzle on the underside of the film. Subsequently, the tape was wound to the mother roll and cut for further testing in 15 mm width.
• Adhesive data Adhesion to steel 2.05 N / cm Unwind force at 0.3 m / min 0.9 N / cm application rate 22 g / m 2
• the film was prepared as an Example 1. As raw material Bormod HD 905 was used. Film properties: failure feature Third colour crystal clear cloudiness 4.5% shine 132.6%
• Adhesive data Adhesion to steel 2.7 N / cm Unwind force at 0.3 m / min 1 N / cm application rate 25 g / m 2 .
• the film was prepared as in Example 1 except that the draw ratio was set at 1: 8.
• a mixture of 98.9 parts by weight of Moplen HP 501 D, 0.9 parts by weight of remainder yellow HG AE 30 and 0.2 parts by weight of BNX BETAPP-N was chosen.
• Film properties Carrier thickness after stretching 60 ⁇ m failure feature b) Impact resistance across 150 mJ / mm 2 colour pearly yellow cloudiness 53% shine 26.1%

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• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
• Laminated Bodies (AREA)
• Adhesive Tapes (AREA)
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• 2006
  • 2006-07-21 DE DE102006044041A patent/DE102006044041A1/de not_active Withdrawn
• 2007
  • 2007-06-28 EP EP07111238A patent/EP1881044A3/fr not_active Withdrawn
  • 2007-06-29 CA CA002593060A patent/CA2593060A1/fr not_active Abandoned
  • 2007-07-18 JP JP2007186939A patent/JP2008024935A/ja active Pending

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